HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → (5-Bromo-2-iodo-benzyl)-ethyl-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Ethylamine | HCID 6341 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Reactant | 5-Bromo-2-iodobenzaldehyde | HCID 21973861 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | (5-Bromo-2-iodo-benzyl)-ethyl-amine | HCID 58148919 | — |
Reaction Steps
To 5-bromo-2-iodo-benzaldehyde (5.0 g, 16.1 mmol) in MeOH (20 mL) was added ethylamine (2M in MeOH; 16 mL, 24.0 mmol), followed by acetic acid (1.0 mL, 17.8 mmol), and the mixture was stirred at room temperature for 30 minutes. Sodium cyanoborohydride (2.0 g, 31.8 mmol) was then added over 5 minutes, and the reaction was stirred at room temperature over the weekend. The mixture was concentrated and partitioned between EtOAc and saturated aqueous NaHCO3. The aqueous layer was extracted with EtOAc, and the combined organic layers were dried over MgSO4, filtered, and concentrated. The residue was purified by silica gel chromatography (0-5% MeOH in CH2Cl2) to give the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08067445B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-621cd2ac909d464b8f9fdee7ed0db861 |
| Source note | uspto-grants-2011_11 |